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Development and validation of a ultra high performance liquid chromatography–tandem mass spectrometric method for the direct detection of formoterol in human urine

Sardela, V.F. ; Deventer, K. ; Pereira, H.M.G. ; de Aquino Neto, F.R. ; Van Eenoo, P.

Journal of pharmaceutical and biomedical analysis, 2012-11, Vol.70, p.471-475 [Periódico revisado por pares]

Amsterdam: Elsevier B.V

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Título:
Development and validation of a ultra high performance liquid chromatography–tandem mass spectrometric method for the direct detection of formoterol in human urine
Autor: Sardela, V.F. ; Deventer, K. ; Pereira, H.M.G. ; de Aquino Neto, F.R. ; Van Eenoo, P.
Assuntos: Acetates - chemistry ; acetic acid ; Acetic Acid - chemistry ; Adrenergic beta-2 Receptor Agonists - urine ; ammonium acetate ; Analysis ; Analytical, structural and metabolic biochemistry ; asthma ; beta-adrenergic agonists ; Biological and medical sciences ; Biomarkers - urine ; Bronchodilator Agents - urine ; bronchodilators ; Calibration ; Chromatography, High Pressure Liquid - standards ; Doping ; Doping in Sports ; Drug Stability ; enzymatic hydrolysis ; Ethanolamines - urine ; Formoterol ; Formoterol Fumarate ; Fundamental and applied biological sciences. Psychology ; General pharmacology ; Humans ; Hydrogen-Ion Concentration ; Hydrolysis ; LC–MS ; liquid chromatography ; Medical sciences ; methanol ; Methanol - chemistry ; Performance-Enhancing Substances - urine ; Pharmacology. Drug treatments ; Reference Standards ; Reproducibility of Results ; Sensitivity and Specificity ; Sport ; sports ; Substance Abuse Detection - methods ; Substance Abuse Detection - standards ; tandem mass spectrometry ; Tandem Mass Spectrometry - standards ; Temperature ; uncertainty ; Urinalysis ; Urine ; Water - chemistry ; β2-Agonist
É parte de: Journal of pharmaceutical and biomedical analysis, 2012-11, Vol.70, p.471-475
Notas: http://dx.doi.org/10.1016/j.jpba.2012.06.042
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Descrição: Formoterol is a long acting β2-agonist and has proven to be a very effective bronchodilating agent. Hence it is frequently applied therapeutically for the treatment of asthma. Because β2-agonists might be misused in sports for the stimulatory effects and for growth-promoting action their use is restricted. Since January 2012, formoterol is prohibited in urinary concentrations higher than 30ng/mL. The objective of this study was to develop and validate a simple and robust ultra high performance liquid chromatographic–tandem mass spectrometric (UHPLC–MS/MS) method for the direct quantification of formoterol in urine. Sample preparation was limited to an enzymatic hydrolysis step after which 2μL was injected in the chromatographic system. Chromatography was performed on a C8-column using gradient conditions. The mobile phase consisted of water/methanol (H2O/MeOH) both containing 0.1% acetic acid (HOAc) and 1mM ammonium acetate (NH4OAc). Calibration curve were constructed between 15 and 60ng/mL. Validation data showed bias of 1.3% and imprecision of 5.4% at the threshold. Ion suppression/enhancement never exceeded 7%. Calculating measurement uncertainty showed proof of applicability of the method. Stability of formoterol was also investigated at 56°C (accelerated stability test) at pH 1.0/5.2/7.0 and 9.5. At the physiological pH values of 5.2 and 7.0, formoterol showed good stability. At pH 1.0 and 9.5 significant degradation was observed.
Editor: Amsterdam: Elsevier B.V
Idioma: Inglês

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Development and validation of a ultra high performance liquid chromatography–tandem mass spectrometric method for the direct detection of formoterol in human urine

Sardela, V.F. ; Deventer, K. ; Pereira, H.M.G. ; de Aquino Neto, F.R. ; Van Eenoo, P.

Amsterdam: Elsevier B.V

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